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#$Date: 2023-09-25 11:33:13 +0300 (Mon, 25 Sep 2023) $
#$Revision: 286500 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/75/8107531.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8107531
loop_
_publ_author_name
'Sithole, Sibusiso A.'
'Malan, Federick P.'
'Katerere, David R.'
'Manicum, Amanda-Lee E.'
_publ_section_title
;
 The crystal structure of fac-tricarbonyl(2-pyridin-2-yl-quinoline-κ2
 N,N′)-(pyrazole-\kN)rhenium(I)nitrate, C20H14N4O3ReNO3
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              685
_journal_page_last               687
_journal_paper_doi               10.1515/ncrs-2023-0152
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C20 H14 N4 O3 Re, N O3'
_chemical_formula_sum            'C20 H14 N5 O6 Re'
_chemical_formula_weight         606.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.267(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9572(2)
_cell_length_b                   9.1568(2)
_cell_length_c                   17.3658(3)
_cell_measurement_reflns_used    23205
_cell_measurement_temperature    153.76(10)
_cell_measurement_theta_max      31.1710
_cell_measurement_theta_min      2.5280
_cell_volume                     2043.84(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      153.76(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -21.00  66.00   0.50    0.15    --   -6.08  57.00  30.00  174
  2  ω     -8.00  69.00   0.50    0.15    --   -6.08  21.00 126.00  154
  3  ω     -5.00  20.00   0.50    0.15    --   -6.08  19.00   0.00   50
  4  ω     -5.00  69.00   0.50    0.15    --   -6.08  19.00 -60.00  148
  5  ω     -5.00  69.00   0.50    0.15    --   -6.08  19.00-180.00  148
  6  ω    -81.00   6.00   0.50    0.15    --   -6.08 -21.00 -40.00  174
  7  ω    -18.00  27.00   0.50    0.15    --   -6.08 -99.00 -90.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0446273000
_diffrn_orient_matrix_UB_12      0.0158973000
_diffrn_orient_matrix_UB_13      0.0267362000
_diffrn_orient_matrix_UB_21      -0.0323041000
_diffrn_orient_matrix_UB_22      0.0145425000
_diffrn_orient_matrix_UB_23      0.0291705000
_diffrn_orient_matrix_UB_31      0.0032209000
_diffrn_orient_matrix_UB_32      -0.0743939000
_diffrn_orient_matrix_UB_33      0.0114051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33676
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.950
_diffrn_reflns_theta_min         2.365
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_description       blade
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+0.0829P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4763
_reflns_number_total             5471
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0152_suppl_001.cif
_cod_data_source_block           shelx
_cod_database_code               8107531
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7644(2) -0.0159(3) 0.39006(16) 0.0209(5) Uani 1 1 d . . . . .
C2 C 0.5794(2) 0.0668(3) 0.33831(16) 0.0204(5) Uani 1 1 d . . . . .
C3 C 0.6361(2) 0.0637(3) 0.49450(16) 0.0194(5) Uani 1 1 d . . . . .
C4 C 0.52059(19) 0.4247(3) 0.39775(15) 0.0178(5) Uani 1 1 d . . . . .
C5 C 0.4399(2) 0.3257(3) 0.37236(18) 0.0239(6) Uani 1 1 d . . . . .
H5 H 0.452647 0.223606 0.376026 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3432(2) 0.3754(3) 0.34245(18) 0.0279(6) Uani 1 1 d . . . . .
H6 H 0.289954 0.307100 0.325583 0.034 Uiso 1 1 calc R U . . .
C7 C 0.3217(2) 0.5257(3) 0.33633(17) 0.0294(6) Uani 1 1 d . . . . .
H7 H 0.255203 0.558552 0.313691 0.035 Uiso 1 1 calc R U . . .
C8 C 0.3966(2) 0.6238(3) 0.36300(17) 0.0269(6) Uani 1 1 d . . . . .
H8 H 0.381192 0.725178 0.360106 0.032 Uiso 1 1 calc R U . . .
C9 C 0.4972(2) 0.5774(3) 0.39498(15) 0.0216(6) Uani 1 1 d . . . . .
C10 C 0.5752(2) 0.6753(3) 0.42536(18) 0.0261(6) Uani 1 1 d . . . . .
H10 H 0.562215 0.777406 0.422933 0.031 Uiso 1 1 calc R U . . .
C11 C 0.6695(2) 0.6248(3) 0.45833(17) 0.0239(6) Uani 1 1 d . . . . .
H11 H 0.721321 0.690662 0.480938 0.029 Uiso 1 1 calc R U . . .
C12 C 0.68892(19) 0.4729(3) 0.45837(15) 0.0171(5) Uani 1 1 d . . . . .
C13 C 0.78958(19) 0.4155(3) 0.49553(15) 0.0174(5) Uani 1 1 d . . . . .
C14 C 0.8607(2) 0.4984(3) 0.54343(17) 0.0258(6) Uani 1 1 d . . . . .
H14 H 0.848679 0.599565 0.550604 0.031 Uiso 1 1 calc R U . . .
C15 C 0.9493(2) 0.4324(3) 0.58066(18) 0.0290(6) Uani 1 1 d . . . . .
H15 H 0.998261 0.487701 0.614011 0.035 Uiso 1 1 calc R U . . .
C16 C 0.9660(2) 0.2858(3) 0.56911(17) 0.0268(6) Uani 1 1 d . . . . .
H16 H 1.026870 0.239267 0.593828 0.032 Uiso 1 1 calc R U . . .
C17 C 0.8924(2) 0.2074(3) 0.52073(16) 0.0218(5) Uani 1 1 d . . . . .
H17 H 0.903429 0.106039 0.513297 0.026 Uiso 1 1 calc R U . . .
C18 C 0.7106(2) 0.3830(3) 0.26962(16) 0.0238(6) Uani 1 1 d . . . . .
H18 H 0.641023 0.416735 0.267870 0.029 Uiso 1 1 calc R U . . .
C19 C 0.7818(2) 0.4342(3) 0.22258(17) 0.0298(7) Uani 1 1 d . . . . .
H19 H 0.770989 0.507325 0.183606 0.036 Uiso 1 1 calc R U . . .
C20 C 0.8712(2) 0.3563(3) 0.24450(18) 0.0271(6) Uani 1 1 d . . . . .
H20 H 0.934878 0.365331 0.223178 0.033 Uiso 1 1 calc R U . . .
N1 N 0.61884(16) 0.3757(2) 0.42703(12) 0.0158(4) Uani 1 1 d . . . . .
N2 N 0.80612(16) 0.2701(2) 0.48409(12) 0.0170(4) Uani 1 1 d . . . . .
N3 N 0.75349(16) 0.2801(2) 0.31747(12) 0.0169(4) Uani 1 1 d . . . . .
N4 N 0.85224(17) 0.2651(2) 0.30150(13) 0.0208(5) Uani 1 1 d . . . . .
H4 H 0.897967 0.203845 0.325261 0.025 Uiso 1 1 calc R U . . .
N5 N 1.07929(19) 0.1526(2) 0.38341(15) 0.0231(5) Uani 1 1 d . . . . .
O1 O 0.80534(16) -0.1221(2) 0.37628(13) 0.0307(5) Uani 1 1 d . . . . .
O2 O 0.51666(16) 0.0040(2) 0.29833(12) 0.0333(5) Uani 1 1 d . . . . .
O3 O 0.60773(15) 0.0082(2) 0.54741(12) 0.0281(4) Uani 1 1 d . . . . .
O4 O 0.99778(15) 0.0773(2) 0.38182(13) 0.0321(5) Uani 1 1 d . . . . .
O5 O 1.15321(18) 0.1328(2) 0.43534(15) 0.0363(5) Uani 1 1 d . . . . .
O6 O 1.08544(16) 0.2463(2) 0.33183(13) 0.0327(5) Uani 1 1 d . . . . .
Re1 Re 0.68730(2) 0.15786(2) 0.40810(2) 0.01422(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Re1 N1 81.24(7) . .
N2 Re1 N1 75.48(8) . .
N2 Re1 N3 83.23(8) . .
C3 Re1 N1 95.94(9) . .
C3 Re1 N3 174.49(9) . .
C3 Re1 N2 91.49(9) . .
C3 Re1 C2 90.15(11) . .
C3 Re1 C1 89.64(11) . .
C2 Re1 N1 102.14(9) . .
C2 Re1 N3 95.06(9) . .
C2 Re1 N2 177.24(9) . .
C2 Re1 C1 83.69(11) . .
C1 Re1 N1 171.88(9) . .
C1 Re1 N3 92.70(9) . .
C1 Re1 N2 98.54(10) . .
C12 N1 Re1 113.20(16) . .
C12 N1 C4 118.7(2) . .
C4 N1 Re1 126.98(17) . .
N4 N3 Re1 124.22(15) . .
C18 N3 Re1 129.76(17) . .
C18 N3 N4 106.0(2) . .
C13 N2 Re1 116.11(16) . .
C17 N2 Re1 124.92(17) . .
C17 N2 C13 119.0(2) . .
O6 N5 O4 119.3(2) . .
O5 N5 O4 120.2(2) . .
O5 N5 O6 120.5(2) . .
N3 N4 H4 124.6 . .
C20 N4 N3 110.8(2) . .
C20 N4 H4 124.6 . .
O3 C3 Re1 178.3(2) . .
N1 C12 C13 117.3(2) . .
N1 C12 C11 122.9(2) . .
C11 C12 C13 119.8(2) . .
N1 C4 C9 120.7(2) . .
N1 C4 C5 121.1(2) . .
C5 C4 C9 118.1(2) . .
C8 C9 C4 119.2(3) . .
C10 C9 C4 118.2(2) . .
C10 C9 C8 122.7(2) . .
N2 C13 C12 115.4(2) . .
N2 C13 C14 121.0(2) . .
C14 C13 C12 123.4(2) . .
O2 C2 Re1 175.8(2) . .
O1 C1 Re1 175.9(2) . .
N3 C18 H18 124.7 . .
N3 C18 C19 110.5(2) . .
C19 C18 H18 124.7 . .
C4 C5 H5 119.7 . .
C6 C5 C4 120.7(2) . .
C6 C5 H5 119.7 . .
C12 C11 H11 120.5 . .
C10 C11 C12 119.0(3) . .
C10 C11 H11 120.5 . .
C9 C8 H8 119.4 . .
C7 C8 C9 121.2(3) . .
C7 C8 H8 119.4 . .
C9 C10 H10 119.8 . .
C11 C10 C9 120.4(2) . .
C11 C10 H10 119.8 . .
C13 C14 H14 120.3 . .
C15 C14 C13 119.3(3) . .
C15 C14 H14 120.3 . .
C8 C7 H7 120.2 . .
C8 C7 C6 119.6(3) . .
C6 C7 H7 120.2 . .
C5 C6 C7 121.1(3) . .
C5 C6 H6 119.4 . .
C7 C6 H6 119.4 . .
C18 C19 H19 127.4 . .
C20 C19 C18 105.2(3) . .
C20 C19 H19 127.4 . .
N2 C17 H17 118.9 . .
N2 C17 C16 122.1(3) . .
C16 C17 H17 118.9 . .
C14 C15 H15 120.2 . .
C16 C15 C14 119.6(3) . .
C16 C15 H15 120.2 . .
N4 C20 C19 107.6(3) . .
N4 C20 H20 126.2 . .
C19 C20 H20 126.2 . .
C17 C16 H16 120.6 . .
C15 C16 C17 118.9(3) . .
C15 C16 H16 120.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 N1 2.224(2) .
Re1 N3 2.193(2) .
Re1 N2 2.157(2) .
Re1 C3 1.920(3) .
Re1 C2 1.921(3) .
Re1 C1 1.925(3) .
O3 C3 1.151(3) .
O1 C1 1.148(3) .
O2 C2 1.154(3) .
O4 N5 1.259(3) .
N1 C12 1.337(3) .
N1 C4 1.384(3) .
O6 N5 1.250(3) .
N3 N4 1.350(3) .
N3 C18 1.330(3) .
N2 C13 1.367(3) .
N2 C17 1.344(3) .
O5 N5 1.243(3) .
N4 H4 0.8800 .
N4 C20 1.341(3) .
C12 C13 1.477(4) .
C12 C11 1.414(4) .
C4 C9 1.431(4) .
C4 C5 1.412(4) .
C9 C8 1.415(4) .
C9 C10 1.403(4) .
C13 C14 1.386(4) .
C18 H18 0.9500 .
C18 C19 1.389(4) .
C5 H5 0.9500 .
C5 C6 1.371(4) .
C11 H11 0.9500 .
C11 C10 1.363(4) .
C8 H8 0.9500 .
C8 C7 1.360(4) .
C10 H10 0.9500 .
C14 H14 0.9500 .
C14 C15 1.383(4) .
C7 H7 0.9500 .
C7 C6 1.405(4) .
C6 H6 0.9500 .
C19 H19 0.9500 .
C19 C20 1.372(4) .
C17 H17 0.9500 .
C17 C16 1.389(4) .
C15 H15 0.9500 .
C15 C16 1.378(4) .
C20 H20 0.9500 .
C16 H16 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Re1 N1 C12 C13 -16.9(3) . . . .
Re1 N1 C12 C11 164.2(2) . . . .
Re1 N1 C4 C9 -161.53(18) . . . .
Re1 N1 C4 C5 20.7(3) . . . .
Re1 N3 N4 C20 -178.57(18) . . . .
Re1 N3 C18 C19 178.34(18) . . . .
Re1 N2 C13 C12 4.0(3) . . . .
Re1 N2 C13 C14 179.8(2) . . . .
Re1 N2 C17 C16 -179.9(2) . . . .
N1 C12 C13 N2 9.1(3) . . . .
N1 C12 C13 C14 -166.6(2) . . . .
N1 C12 C11 C10 0.3(4) . . . .
N1 C4 C9 C8 178.5(2) . . . .
N1 C4 C9 C10 -2.3(4) . . . .
N1 C4 C5 C6 -179.1(3) . . . .
N3 N4 C20 C19 0.2(3) . . . .
N3 C18 C19 C20 0.0(3) . . . .
N2 C13 C14 C15 -0.5(4) . . . .
N2 C17 C16 C15 0.9(4) . . . .
N4 N3 C18 C19 0.1(3) . . . .
C12 N1 C4 C9 5.3(4) . . . .
C12 N1 C4 C5 -172.5(2) . . . .
C12 C13 C14 C15 174.9(3) . . . .
C12 C11 C10 C9 2.7(4) . . . .
C4 N1 C12 C13 174.5(2) . . . .
C4 N1 C12 C11 -4.3(4) . . . .
C4 C9 C8 C7 1.2(4) . . . .
C4 C9 C10 C11 -1.7(4) . . . .
C4 C5 C6 C7 -0.1(5) . . . .
C9 C4 C5 C6 3.1(4) . . . .
C9 C8 C7 C6 1.8(4) . . . .
C13 N2 C17 C16 -0.8(4) . . . .
C13 C12 C11 C10 -178.5(3) . . . .
C13 C14 C15 C16 0.6(4) . . . .
C18 N3 N4 C20 -0.2(3) . . . .
C18 C19 C20 N4 -0.1(3) . . . .
C5 C4 C9 C8 -3.6(4) . . . .
C5 C4 C9 C10 175.5(3) . . . .
C11 C12 C13 N2 -172.1(2) . . . .
C11 C12 C13 C14 12.3(4) . . . .
C8 C9 C10 C11 177.4(3) . . . .
C8 C7 C6 C5 -2.4(5) . . . .
C10 C9 C8 C7 -177.8(3) . . . .
C14 C15 C16 C17 -0.7(4) . . . .
C17 N2 C13 C12 -175.1(2) . . . .
C17 N2 C13 C14 0.7(4) . . . .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{dc179565-52fe-4f05-b5fa-09270e9d3599} ? ? ?
{c190dc34-9361-44f2-aebc-c237083a4b02} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{dc179565-52fe-4f05-b5fa-09270e9d3599} '_publcif_info_datablock.publ_exptl'
loop_
_publcif_info_cif.paper_type
CE
;
;
